Hydrochloric Acid → HCID 25417233, Verbindung

HRID 1172044Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1172044
[Br:1][C:2]1[CH:13]=[CH:12][C:5]([C@@H:6]([CH2:8][C:9]([OH:11])=[O:10])[NH2:7])=[CH:4][CH:3]=1.[OH-].[Na+].[C:16](OC(=O)C)(=[O:18])[CH3:17].Cl>O>[C:16]([NH:7][C@H:6]([CH2:8][C:9]([OH:11])=[O:10])[C:5]1[CH:4]=[CH:3][C:2]([Br:1])=[CH:13][CH:12]=1)(=[O:18])[CH3:17]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 14798Sodium Hydroxide2×HCID 724054(r)-3-(p-Bromophenyl)-beta-alanine

Produkt 1

HCID 25417233HCID 25417233, VerbindungAusbeute 102,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

p-Bromo-β-phenylalanine (10.0 g, 41 mmol) was mixed with 40 ml of water and adjusted to pH 14 with 25% sodium hydroxide aqueous solution. After being cooled to 5° C., 8.5 ml of acetic anhydride (90 mmol) and 25% sodium hydroxide aqueous solution were simultaneously dropped into the mixture to keep it at a pH range of 11.5˜12 and the resulting mixture was stirred for 3 hours at a room temperature. After the mixture was adjusted to pH 2 with conc. HCl and stirred for one hour, the resulting precipitated crystal was filtered and dried under reduced pressure to give quantitatively 12.0 g of acetyl-p-bromo-β-phenylalanine.

Aufarbeitung

  1. stirringstirred for one hour
  2. customthe resulting precipitated crystal
  3. filtrationwas filtered
  4. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-ecdb8b282c9b4a18b0ab8f6b25fbb478
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07833760B2

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